In the past, meso-nordihydroguaiaretic acid, (N.D.G.A.), expensively derived from Larrea divaricata or Larrea tridentata, the creosote bush, or snythesized from phenyl ethers, has been used as a food additive and anti-oxidant. Optically active N.D.G.A. and racemic mixtures thereof are also useful for this purpose. The d,1-form, as distinguished from the meso-form, gives a pleasant odor to soaps and toilet articles; and is more soluble than its meso isomer. The optically active N.D.G.A. (and racemic mixture thereof) of this invention is distinguished from the meso form by its melting point of 157.degree. C. to 160.degree. C., as opposed to the 185.degree. C. to 186.degree. C. melting point of the meso form. Racemic 2,3-dimethyl,1,4-bis(3,4-dimethoxyphenyl)-1,4-butanedione has served as an intermediary in the synthesis of meso-N.D.G.A. in prior art processes, but the optical orientation of the 2,3-dimethyl bonds has been lost in subsequent processing steps. This invention involves the preservation of the optical orientation of these bonds through reduction, methylation and cleavage steps to produce optically active molecules, or a racemic mixture of N.D.G.A., as well as the diols and ethers intermediate to the synthesis. Insofar as the optically active isomers and racemic mixture of N.D.G.A. may be utilized in place of the meso form thereof, the synthesis of d,1-N.D.G.A. provided herein fulfills the need for an easier, less expensive method of production, providing product in higher yields than prior art processes, without the use of high pressure hydrogenation equipment and expensive catalysts.